CN108555428A - A kind of preparation method and application of metal-based nano composite solder - Google Patents
A kind of preparation method and application of metal-based nano composite solder Download PDFInfo
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- CN108555428A CN108555428A CN201810530674.0A CN201810530674A CN108555428A CN 108555428 A CN108555428 A CN 108555428A CN 201810530674 A CN201810530674 A CN 201810530674A CN 108555428 A CN108555428 A CN 108555428A
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
- Manufacturing Of Electrical Connectors (AREA)
Abstract
The invention belongs to superconducting tape welding technology fields, are related to a kind of preparation method and application of metal-based nano composite solder, the preparation method more particularly, to a kind of metal-based nano composite solder and its application in the welding of yttrium system high-temperature superconducting body.Nano metal Argent grain is disperseed using metal indium gallium alloy, the welding material used when the welding of yttrium based high-temperature superconductive strip is made, while forming diffused interconnections structure using metallic silver corpuscle low-temperature sintering, metal Nano silver grain can be dispersed in rough surface to be welded by the mobility of low-temperature metal indium gallium alloy again.The method of the invention significantly improves the contact area between nano silver composite solder and face of weld, and then obtains low resistance interface, and improves the weld strength at interface.
Description
Technical field
The invention belongs to superconducting tape welding technology field, be related to a kind of metal-based nano composite solder preparation method and
Using a kind of, preparation method more particularly, to metal-based nano composite solder and its in the welding of yttrium system high-temperature superconducting body
Application.
Background technology
Yttrium system high-temperature superconducting body has extremely excellent superconductivity energy under liquid nitrogen temperature (77K), thus is sent out in superconduction
The field of strong electricity such as motor, superconductive current limiter, superconducting transformer and superconducting magnet energy-storage system have great application potential.So
And be limited to the complicated technology of multicoating, deposition film uniformity be difficult to control and final finished rate still it is more low it is many because
Element, the economy for preparing long band at present be not high.Therefore, meet the length in practical application by connecting relatively short band
Demand is particularly important the application scenarios such as large-scale magnet and long distance powedr transmission.
Currently, the connection of yttrium based high-temperature superconductive strip mainly uses solder mode, i.e., by melting low temperature scolding tin (slicker solder
Solder or indium) solder come realize superconducting tape connect；This technical process is simple and can be connect by increasing overlapping area to reduce
Head resistance is the current main welding technique for obtaining low resistance hts band connector.However, scolding tin and superconducting tape metal
The interface of protective layer (copper Cu or silver Ag) does not form that metallurgical binding, there are contact resistances, it will usually lead to soldered fitting
Resistance is larger and low-temperature welding intensity is poor (even if using the good high lead class solder of low-temperature flexibility, weld strength is still poor).
Dimensional effect based on nano-Ag particles, i.e., at a lower temperature metallic silver corpuscle can occur melting and it is interparticle
Atom phase counterdiffusion, can be under the conditions of short time (2~20min) and low temperature (100~200 DEG C), in yttrium system high-temperature superconducting band
Metallic silver diffused interconnections structure is formed at material weld interface, can get low resistance welding point.However, nano silver particles usually divide
It is dispersed in low boiling point dispersant, when use need to be coated in metal surface to be welded repeatedly, pass through heating again after the solvent is volatilized
Mode implement to weld.The dosage that this technical process is excessively cumbersome and nano silver particles are in solder is not easy to control；Especially exist
During solvent volatilizees, nano silver particles occur hardened, it may be difficult to it is dispersed into the rough surface of metal to be welded well,
And then influence the interface cohesion between silver solder and metal to be welded.
Accordingly, it is desirable to provide a kind of new brazing metal, is used for low resistance yttrium system high-temperature superconducting body welding point, to solve
Above-mentioned technical problem.
Invention content
It is an object of the present invention to provide a kind of Metal Substrate for the welding point of low resistance yttrium system high-temperature superconducting body to receive
Rice composite solder；Another is designed to provide a kind of welding side of the low resistance yttrium system high-temperature superconducting body based on nanometer silver solder
Method realizes that the short time of yttrium based high-temperature superconductive strip heats welding process, it is ensured that the performance of superconducting tape is unaffected；Meanwhile
Welding point resistance is low, satisfactory mechanical property, high yield rate.
In order to achieve the above objectives, the present invention uses following technical proposals：
A kind of preparation method of metal-based nano composite solder, includes the following steps：
A, after being uniformly mixed sodium citrate solution and deionized water, then silver nitrate aqueous solution is added in heating；
B, in the mixed solution of above-mentioned preparation, sodium borohydride solution is added, is first vigorously stirred, is then gradually cooling to room
Temperature obtains the dispersed nano silver colloidal solution S1 that grain size is 5nm；
C, under conditions of being vigorously stirred, S1 solution is first added to the solution of sodium citrate solution and deionized water mixing
In, silver nitrate aqueous solution is added, is stirred, room temperature is then gradually cooling to, obtains the dispersed nano that average grain diameter is 20nm
Silver colloidal solution S2；
D, the processing procedure described in step C is used to prepare average grain diameter as the dispersed nano elargol of 30nm S2 solution
Liquid solution S3；
E, step C is repeated to the solution S of acquisition 3, until finally obtaining the dispersed nano that average grain diameter is 5~80nm
Elargol dispersion liquid；
F, the single dispersed nano silver colloidal dispersion obtained in step E is centrifuged, obtains nano-Ag particles；
G, first metal indium gallium alloy is heated and is melted, form liquid metal, the nano-Ag particles for then obtaining step F
It is added into above-mentioned liquid metal and uniformly mixes, metal-based nano composite solder is prepared.
Based on the above technical solution, a concentration of 10g/L of sodium citrate solution described in step A and step C；Step
A concentration of 1g/L of sodium borohydride solution described in rapid B；A concentration of 10g/ of silver nitrate aqueous solution described in step A and step C
L。
Based on the above technical solution, the volume of sodium citrate solution described in step A is 1L, the silver nitrate water
The volume of solution is 85mL, and the volume of the deionized water is 3.75L；The volume of sodium borohydride solution described in step B is
100mL；The volume of S1 solution described in step C is 2L, and the volume of the sodium citrate solution is 400mL, the deionized water
Volume be 1.5L, the volume of the silver nitrate aqueous solution is 340mL.
Based on the above technical solution, in the step A, sodium citrate solution and deionized water are stirred
After uniformly, it is heated to 80 DEG C；It is vigorously stirred described in step B and C and is carried out at a temperature of 80 DEG C.
Based on the above technical solution, the duration being vigorously stirred described in step B is 1.5h；Described in step C
The duration of stirring is 1.5h.
Based on the above technical solution, the volume ratio of nano-Ag particles and metal indium gallium alloy described in step G is
5/95~80/20.
Based on the above technical solution, the operation described in step A-E is carried out in a kettle；After centrifugation
Processing is dried in the nano-Ag particles of acquisition.
A method of welding yttrium system high-temperature superconducting body connector, including following step using above-mentioned metal-based nano composite solder
Suddenly：
A, to two bands made of yttrium system high-temperature superconducting body material, the connector table that needs weld close to superconducting layer side
Face is polished, to remove the oxide layer of metal surface；
B, metal-based nano composite solder is positioned on the surface after polishing,
C, the side surface after first above-mentioned two bands being polished is bonded, and is then heated, is carried out pressure welding.
Based on the above technical solution, the condition of the pressure welding is：Temperature is 100~200 DEG C, positive pressure
For 0.1~2MPa, the retention time is 2~20min.
Based on the above technical solution, in step a, the joint surface welded to needs using sand paper is beaten
Mill；Before the step b, the surface after being polished with alcohol rinse.
The advantageous effects of the present invention are as follows：
The present invention disperses nano metal Argent grain using metal indium gallium alloy, makes when the welding of yttrium based high-temperature superconductive strip is made
Welding material, while forming diffused interconnections structure using metallic silver corpuscle low-temperature sintering, and can be by low-temperature metal
Metal Nano silver grain is dispersed in rough surface to be welded, it is compound to be remarkably improved nano silver by the mobility of indium gallium alloy
Contact area between solder and face of weld, and then obtain low resistance interface and (reach 10-9Ω grades), and the welding for improving interface is strong
Degree (from common 70MPa improve to>100MPa).
Description of the drawings
The present invention has following attached drawing：
Fig. 1 shows that the low resistance interface formed when metal-based nano composite solder is applied to the welding of yttrium system high-temperature superconducting body is shown
It is intended to；
Fig. 2 shows the stereoscan photographs on surface and compact area after welding.
Reference numeral：1 silver medal (copper) stabilized zone, 2 layers
Specific implementation mode
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and not restrictive, should not be limited the scope of the invention with this, and specific technical solution is such as
Under.
A kind of preparation method of metal-based nano composite solder, includes the following steps：
A, after being uniformly mixed sodium citrate solution and deionized water, then silver nitrate aqueous solution is added in heating；
B, in the mixed solution of above-mentioned preparation, sodium borohydride solution is added, is first vigorously stirred, is then gradually cooling to room
Temperature obtains the dispersed nano silver colloidal solution S1 that grain size is 5nm；
C, under conditions of being vigorously stirred, S1 solution is first added to the solution of sodium citrate solution and deionized water mixing
In, silver nitrate aqueous solution is added, is stirred, room temperature is then gradually cooling to, obtains the dispersed nano that average grain diameter is 20nm
Silver colloidal solution S2；
D, the processing procedure described in step C is used to prepare average grain diameter as the dispersed nano elargol of 30nm S2 solution
Liquid solution S3；
E, step C is repeated to the solution S of acquisition 3, until finally obtaining the dispersed nano that average grain diameter is 5~80nm
Elargol dispersion liquid；
F, the single dispersed nano silver colloidal dispersion obtained in step E is centrifuged, obtains nano-Ag particles；
G, first metal indium gallium alloy is heated and is melted, form liquid metal, the nano-Ag particles for then obtaining step F
It is added into above-mentioned liquid metal and uniformly mixes, metal-based nano composite solder is prepared.
Based on the above technical solution, a concentration of 10g/L of sodium citrate solution described in step A and step C；Step
A concentration of 1g/L of sodium borohydride solution described in rapid B；A concentration of 10g/ of silver nitrate aqueous solution described in step A and step C
L。
Based on the above technical solution, the volume of sodium citrate solution described in step A is 1L, the silver nitrate water
The volume of solution is 85mL, and the volume of the deionized water is 3.75L；The volume of sodium borohydride solution described in step B is
100mL；The volume of S1 solution described in step C is 2L, and the volume of the sodium citrate solution is 400mL, the deionized water
Volume be 1.5L, the volume of the silver nitrate aqueous solution is 340mL.
Based on the above technical solution, in the step A, sodium citrate solution and deionized water are stirred
After uniformly, it is heated to 80 DEG C；It is vigorously stirred described in step B and C and is carried out at a temperature of 80 DEG C.
Based on the above technical solution, the duration being vigorously stirred described in step B is 1.5h；Described in step C
The duration of stirring is 1.5h.
Based on the above technical solution, the volume ratio of nano-Ag particles and metal indium gallium alloy described in step G is
5/95~80/20.
Based on the above technical solution, the operation described in step A-E is carried out in a kettle；After centrifugation
Processing is dried in the nano-Ag particles of acquisition.
A method of welding yttrium system high-temperature superconducting body connector, including following step using above-mentioned metal-based nano composite solder
Suddenly：
A, to two bands made of yttrium system high-temperature superconducting body material, the connector table that needs weld close to superconducting layer side
Face is polished, to remove the oxide layer of metal surface；
B, metal-based nano composite solder is positioned on the surface after polishing,
C, the side surface after first above-mentioned two bands being polished is bonded, and is then heated, is carried out pressure welding.
Based on the above technical solution, the condition of the pressure welding is：Temperature is 100~200 DEG C, forward direction pressure
Power is 0.1~2MPa, and the retention time is 2~20min.
Based on the above technical solution, in step a, the joint surface welded to needs using sand paper is beaten
Mill；Before the step b, the surface after being polished with alcohol rinse.
Embodiment
A kind of preparation method of metal-based nano composite solder, includes the following steps：
(1) preparation of nanometer silver solder：The sodium citrate solution of a concentration of 10g/L of 1L and 3.75L deionized waters are stirred
In a kettle after mixing, 80 DEG C are heated to, then the silver nitrate aqueous solution of a concentration of 10g/L of 85mL is added above-mentioned
In reaction kettle.
The sodium borohydride solution of a concentration of 1g/L of 100mL is rapidly joined in above-mentioned reaction system, at a temperature of 80 DEG C,
It is vigorously stirred 1.5h, is then gradually cooling to room temperature, obtains the dispersed nano silver colloidal solution S1 that grain size is 5nm.
In reaction kettle under the conditions of 80 DEG C of high degree of agitation, the S1 solution of 2L is first added to a concentration of 10g/L of 400mL
In sodium citrate solution and the solution of 1.5L deionized waters mixing.The silver nitrate aqueous solution of a concentration of 10g/L of 340mL is added again
In reaction kettle, 1.5h is stirred, is then gradually cooling to room temperature, obtains the single dispersed nano silver colloidal dispersions that average grain diameter is 45nm
Liquid is centrifuged and is dried to the single dispersed nano silver colloidal dispersion of above-mentioned acquisition, obtains single dispersed nano silver
Particle.
(2) preparation of metal-based nano composite solder：First metal indium gallium alloy is heated and is melted, fused solution gold is formed
Belong to, then the dispersed nano Argent grain that grain size is 45nm is added into fused solution metal and is uniformly mixed, Metal Substrate is made
The volume ratio of nanocomposite solders, the nano-Ag particles and metal indium gallium alloy is 80/20.
Yttrium based high-temperature superconductive strip is welded using above-mentioned metal-based nano composite solder, chooses two metal copper-clads
It seals, (liquid nitrogen temperature 77K is in use, self-fields critical current is I to the yttrium based high-temperature superconductive strip of 12mm widec=300A), use sand paper
Band polish close to the metallic copper cover surface of superconducting layer side, removes the oxide layer of metal surface；It is polished with alcohol rinse
Surface, polishing length are 3cm, metal-based nano composite solder are placed on buffed surface, and by two superconducting tapes close to superconduction
One side surface of layer fits together, be subsequently placed in the welding fixture locating slot that temperature is 150 DEG C, positive pressure is 1MPa,
10min pressure welding is kept, the welding of the low resistance yttrium system high-temperature superconducting body based on nanometer silver solder is finally completed, forms welding
Connector, the connection resistance under 77K, which reaches, receives Europe grade (10-9Ω), shearing strength of joint reaches 115MPa, and after welding, band faces
Boundary electric current IcIt remains unchanged, welding situation is as depicted in figs. 1 and 2, the silver (copper) of two yttriums based high-temperature superconductive strip shown in Fig. 1
Layer 2 is formed between stabilized zone 1.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate examples of the invention, and is not pair
The restriction of embodiment of the present invention for those of ordinary skill in the art on the basis of the above description can be with
It makes other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to the present invention
Technical solution changes and variations that derived from still in protection scope of the present invention row.
The content not being described in detail in this specification belongs to the prior art well known to professional and technical personnel in the field.
Claims (10)
1. a kind of preparation method of metal-based nano composite solder, it is characterised in that：Include the following steps：
A, after being uniformly mixed sodium citrate solution and deionized water, then silver nitrate aqueous solution is added in heating；
B, in the mixed solution of above-mentioned preparation, sodium borohydride solution is added, is first vigorously stirred, is then gradually cooling to room temperature,
Obtain the dispersed nano silver colloidal solution S1 that grain size is 5nm；
C, under conditions of being vigorously stirred, first S1 solution is added in sodium citrate solution and the solution of deionized water mixing,
Silver nitrate aqueous solution is added, is stirred, room temperature is then gradually cooling to, obtains the dispersed nano elargol that average grain diameter is 20nm
Liquid solution S2；
D, the processing procedure described in step C is used to prepare average grain diameter as the dispersed nano silver colloidal solution of 30nm S2 solution
S3；
E, step C is repeated to the solution S of acquisition 3, until finally obtaining the dispersed nano silver colloid that average grain diameter is 5~80nm
Dispersion liquid；
F, the single dispersed nano silver colloidal dispersion obtained in step E is centrifuged, obtains nano-Ag particles；
G, first metal indium gallium alloy is heated and is melted, formed liquid metal, be then added into the step F nano-Ag particles obtained
It is uniformly mixed in above-mentioned liquid metal, metal-based nano composite solder is prepared.
2. the preparation method of metal-based nano composite solder as described in claim 1, it is characterised in that：In step A and step C
A concentration of 10g/L of the sodium citrate solution；A concentration of 1g/L of sodium borohydride solution described in step B；Step A and step
A concentration of 10g/L of silver nitrate aqueous solution described in C.
3. the preparation method of metal-based nano composite solder as claimed in claim 2, it is characterised in that：Lemon described in step A
The volume of lemon acid sodium solution is 1L, and the volume of the silver nitrate aqueous solution is 85mL, and the volume of the deionized water is 3.75L；
The volume of sodium borohydride solution described in step B is 100mL；The volume of S1 solution described in step C is 2L, the sodium citrate
The volume of solution is 400mL, and the volume of the deionized water is 1.5L, and the volume of the silver nitrate aqueous solution is 340mL.
4. the preparation method of metal-based nano composite solder as described in claim 1, it is characterised in that：In the step A,
After sodium citrate solution and deionized water are uniformly mixed, it is heated to 80 DEG C；It is vigorously stirred 80 described in step B and C
It is carried out at a temperature of DEG C.
5. the preparation method of metal-based nano composite solder as described in claim 1, it is characterised in that：Described in step B acutely
The duration of stirring is 1.5h；The duration stirred described in step C is 1.5h.
6. the preparation method of metal-based nano composite solder as described in claim 1, it is characterised in that：It is received described in step G
The volume ratio of rice Argent grain and metal indium gallium alloy is 5/95~80/20.
7. the preparation method of metal-based nano composite solder as described in claim 1, it is characterised in that：It carries out in a kettle
Operation described in step A-E；To the nano-Ag particles obtained after centrifugation, processing is dried.
8. gold prepared by a kind of preparation method using metal-based nano composite solder described in claim 1-7 any claims
Belong to the method for base nanocomposite solders welding yttrium system high-temperature superconducting body connector, it is characterised in that：Include the following steps：
A, to two bands made of yttrium system high-temperature superconducting body material, close to superconducting layer side need the joint surface welded into
Row polishing, to remove the oxide layer of metal surface；
B, metal-based nano composite solder is positioned on the surface after polishing,
C, the side surface after first above-mentioned two bands being polished is bonded, and is then heated, is carried out pressure welding.
9. the method for welding yttrium system high-temperature superconducting body connector as claimed in claim 8, it is characterised in that：The pressure welding
Condition is：Temperature is 100~200 DEG C, and positive pressure is 0.1~2MPa, and the retention time is 2~20min.
10. the method for welding yttrium system high-temperature superconducting body connector as claimed in claim 8, it is characterised in that：In step a, make
The joint surface welded to needs with sand paper is polished；Before the step b, the surface after being polished with alcohol rinse.
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| CN110102934A (en) * | 2019-04-30 | 2019-08-09 | 周轻轩 | A kind of preparation method of electrochemically resistant migration-type nano silver composite solder paste material |
| CN110773859A (en) * | 2019-11-04 | 2020-02-11 | 深圳市汇城精密科技有限公司 | Method for welding metal materials |
| CN111009798A (en) * | 2019-12-20 | 2020-04-14 | 中国科学院电工研究所 | Multi-core iron-based superconducting joint and preparation method thereof |
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